chopor
DISTILLATION
Distillation is an unit operation in which constituents of liquid mixture (solution) are
separated using thermal energy. Basically, the difference in vapour pressure of different
constituents at the same temperature is responsible for such separation. This unit operation
js also termed as fractional distillation or fractionation. With this technique it is possible
to separate liquid mixture into its components in almost pure form and this fact has made
distillation perhaps the most important of all mass transfer operations.
In distillation, the phases involved are liquid and vapour or gas (vapour phase is
created by supplying heat to liquid) and mass is transferred from both the phases to one
another, by vaporisation from liquid phase and by condensation from vapour phase. The
basic requirement for separation of components by distillation is that the composition of
vapour be different from the composition of the liquid with which it is in equilibrium. The
vapour is always richer in the more volatile component than the liquid from which it is
formed. If the vapour composition is same as the liquid composition, distillation technique
will not effect a separation.
Distillation is commonly encountered in chemical and petroleum industries as a
means of separating the liquid mixture into its component parts. Separation of ethanol and
water mixture, production of absolute alcohol from 95% ethyl alcohol using benzene,
separation of petroleum crude into gasoline, kerosene, fuel oil ete. are the typical examples
of distillation.
Evaporation is concerned with separation of solution containing non-volatile solute
and volatile solvent whereas distillation is concerned with separation of solutions where
all the components are appreciably volatile. Thus, the separation of a brine into salt and
water is a evaporation whereas the separation of a mixture of alcohol and water into its
components is a distillation.
Boiling Point :
For any given pressure, a pure liquid when heated will boil or vaporise at a certain
single temperature known as boiling point of the liquid. Boiling point of a liquid increases
with inerease in pressure and vice versa. Boiling points at a given pressure vary greatly
for different liquids. For example, boiling point of water is 373 K (100° C), that of toluene is
383.6 K (110.6° C) and that of methanol is 337.7 K (64.79) at one atmosphere
(101.325 kPa).
In the binary mixture (two component system), the component with lower boiling point
or component with higher vapour pressure at a given temperature, is termed as more
volatile or lighter and the component with higher boiling point or with lower vapour
pressure at a given temperature is termed as less volatile or heavier.
Thus in case of binary mixture of methanol and water, methanol is more volatile
component and water is less volatile component. The whole mixture of methanol and water
will boil somewhere between 337.7 K (64.7° C) and 378 K (100°C) at atmospheric pressure
(101.325 kPa).
(1.1)Mass Transfer ~ Il 1.5 Distillation
Majority of distillation operations are carried out at constant total pressure. For
distillation calculations, the equilibrium vapour-liquid composition can also be plotted as
shown in Fig. 1.2 wherein vapour phase composition (y) is plotted as ordinate and liquid
phase composition (x) is plotted as abscissa. Such a diagram is called as an equilibrium
diagram or distribution diagram. As the vapour is richer in more volatile component than
the liquid, the equilibrium curve lies above the 45° diagonal line which is drawn for
comparison.
10
‘Temperature —__»
0,0 xy —> 1.0 0.0 x 1.0
J Fig. 1.8: Effect of increased pressure : vapour-liquid equilibrium
~ Raoult's law:
It is commonly used for predicting vapour-liquid equilibrium for an ideal solution in
equilibrium with an ideal gas mixture from vapour-pressure data. It states that
equilibrium partial pressure of a constituent at a given temperature is equal to the product
of its vapour pressure in a pure state and its mole fraction in the liquid phase.
‘Thus, for a binary (two component) system, if pa is the equilibrium partial pressure of
A, p® is the vapour pressure of A in pure state and xq is the mole fraction of A in the liquid
phase, then,
PA = PA Xa ala)
and Pp = PS Xp (EQ)
= pp (1-xq), as xa +xp=1
where Pp = equilibrium partial pressure of B
Xp = mole fraction of B in liquid phase
a pe = vapour pressure of pure B.
~Dalton's law :
It states that the total pressure exerted by a gas/vapour mixture is equal to the sum of the
partial pressures of the components present in it. Thus, it expresses the additive nature of
partial pressures.
Mathematically, for a binary system :
P = patps (18)
where P is the total pressure.Mass Transfer — II 1.6 Distillation
For ideal gas or vapour, the partial pressure is related to the mole fraction of the
component in the gas or vapour phase by the relation ;
Partial pressure = Mole fraction x Total pressure
Thus, for component A,
Pa = ya'P + (4)
where ya is the mole fraction of A in the vapour phase.
Knowing the vapour pressures of components A (more volatile) and B at various values
of temperatures, x - y data can be generated for an ideal solution as follows :
Pa = Py *Xa + (1.5)
Pp = Py‘ (1—xa) «+ (1.6)
Pa = Ya’ P oe (L7)
Pp = Ya'P w+ (8)
From Equations (1.5) and (1.7), we get
Po°Xs = Yas P + (1.9)
Pe
ya = Bom -+- (1.10 a)
o
Similarly, ye = ee “xp w+ (1.10 b)
But Yo+Yp = land xp= 1-x,
YatYe = 1 oe (1.11)
Putting values of y, and yg from Equations (1.10) and (1.11), and of xp in terms of xa,
in Equation (1.11), we get,
° °
P,
? me (l-x) = 1 spafl «+ (L.15)
PAT PB
_/ Knowing xa, corresponding equilibrium value of the vapour phase concentration (yq)
As obtained with the help of Equation (1.10 a).
Relative volatility :
Volatility of A : It is defined as the ratio of the partial pressure of A to the mole fraction
of A in the liquid phase.
‘ = Pa
Volatility of A = XA ++ (1.16)
Similarly, Volatility of B = Pa w- (1.17)Mass Transfer ~ Il A. Distillation,
Relative volatility is the ratio of the volatility of A (more volatile component) to that of
B. It is also known as volatility of A with respect to B and is denoted by a symbol cap.
_ PaXs
Gan = xepe - (1.18)
but Pya = Pa and Pyg=Pp
_ YaXs
Gan = xe + (1.19)
_ Ya/Yp
Gan = tap .-- (1.20)
‘Thus, relative volatility is the ratio of concentration ratio of A to B in the vapour phase
to that in the liquid phase.
Yas
cap = VASB
ee
We have, yp = 1-¥a se L201)
Xp = 1-x, ++. (1.22)
_ Ya(l- xa) ic
Op = howe % .- (1.28)
Gap (1—ya)Xq = ya (1—¥,)
Gap Xa~ Cap YaXa = Ya—YaXa
Gap XA = YatYaXa (Gap - 1)
GapXa = yall +(Gap—D xal
eyes TAB ZA
Ya = T+(ap-D¥a + (24)
Dropping subseript, we get :
ox 3
y= ves (1.25)
_ g-9)
« = Yay (1.26)
From Equation (1.25), knowing « for a given binary system, x - y data (equilibrium
data) can be generated by taking x = 0, 0.1...... to 1 and evaluating corresponding values of
y (equilibrium vapour phase composition).
For ideal system, the volatility is equal to the vapour pressure of the pure component.
‘Therefore, the relative volatility of two substances forming an ideal solution is the
ratio of their vapour pressures.
v
Relative volatility =o4g=a = ~% w= (L272)
Pa
Relative volatility is a measure of separability by distillation and when a = 1
separation by distillation is not possible. Separation by distillation is possible for relative
volatility values greater than one. Larger the value of relative volatility, easier is the
separation by distillation.Mass Transfer — I! 1.8 Distillation
‘THE METHODS OF DISTILLATION - BINARY SYSTEMS :
Basically, distillation is carried out in two ways :
1, The liquid mixture is heated to create vapour. The vapours formed are condensed
in a condenser and withdrawn as a product. As there is no reflux, the products of relatively
low purities are obtained.
2. The liquid mixture is heated to create vapour, vapours formed are condensed in the
condenser. Part of the condensed liquid is returned to the distillation system (as reflux)
and the remaining part is withdrawn as a product. In this, liquid and vapour are brought
into intimate contact for a number of times and almost pure product can be achieved and
the operation is called rectification or fractionation: The term rectification originated in
alcohol industry whereas the term fractionation is popular in petroleum industry.
Common methods used in distillation practice are :
1. Differential or simple distillation,
2. Flash or equilibrium distillation,
3. Rectification or fractionation.
Out of these three methods, distillation with rectification or simply called rectification
is the most important. The first two methods are carried out without reflux and the third one
is carried out with reflux (- which is nothing but returning a part of the condensed liquid
bagk to the distillation system).
Misc or Simple Distillation :
In this distillation technique, a known quantity of liquid mixture is charged into a
jacketed kettle or still. The jacket is provided for heating the mass in the still with the help
of a heating media such as steam. The charge is boiled slowly, vapours formed are
withdrawn and fed to a condenser where they are liquified and collected in the receiver as
a distillate. In early stage of distillation, vapours leaving the still are richest in the more
volatile component and as the distillation proceeds the liquid in the still becomes lean with
Vapour
Coolant
out
Feed
(Condenser
Coolant
in
Still/kettle
lacketed)
R
‘Condensate R,R, - Distillate receivers
Residue
~~ Fig. 1.4 : Simple distillation unitee eee ee
Mass Transfer ~ Il
1.9 ab Distillation
respect to more volatile component. The composition of the less volatile component thereby
increases and hence the boiling point increases. The product (distillate) from such units
can be collected in several receivers, called cuts, to give products of various purities over
the length of distillation period. The distillation is continued till the boiling point of liquid
reaches a predetermined valué and the content of the still is‘finally removed as residual
liquid containing majority of less volatile component.
prea balance - binary mixtures :
N ‘As the composition of vapour issuing from distillation and that of the liquid remaining
in it changes during the course of operation, the mathematical approach should be
differential.
Let F be the kmol of liquid mixture (A + B) containing xp mole fraction of A which is
charged to distillation still. Let D be kmol of distillate and W be kmol of residual liquid in
still which are obtained at the end of operation. Let ypavg and xw be the mole fraction of A
in distillate and bottom residual liquid.
Let L be the kmol of liquid in the still at any time during the course of distillation and
let x be the mole fraction of A in liquid, Let very small amount dD kmol of the distillate of
. the composition y in equilibrium with the liquid is vaporised. Then the composition and
quantity of liquid decreases from x to x — dx and L to L-dL respectively.
Then,
Overall material balance at any time is :
L = L-db+aD «++ (1.28)
" aL = aD ... (1.29)
Material balance of component A
Lx = (L-dL)(x-dx)+y aD «.- (1.80)
Lx = Lx-Lédx-xdL +dLdx + ydD
dLdx being very small can be neglected.
0 = -Ldx-xdL + ydD (13D)
Put the value of dD as dL from Equation (1.29)
0 = - Ldx—xdL + yd .. (1.32)
Lex = (y-x) dL .. (1.33)
aL _ dx
FP joe (1.34)
4 Integrating the above equation between two extreme conditions :
L=F, x=x
and L = W, x=3w
F xP
aL dx
Je- fes ws (1.35)
xw
XP
F dx
n& = Js «.. (1.86)
xw
(y is in equilibrium with x i.e. y is the vapour phase composition in equilibrium with
liquid phase composition (x)).Mass Transfer ~ I| 1.10 Distillation
Equation (1.36) is known as the Rayleigh equation. It is used to determine F, W, xp or
xw when three of these are known. RHS of Equation (1.36) i.e. integral on the RHS side is
evaluated graphically by plotting 1y — x) as an ordinate and x as the abscissa and
determining the area under the curve between x = xp and x= xw. The required data for
above procedure are taken from vapour-liquid equilibrium relationship.
Ifyp, avg, is a composition of composited distillate, then,
Material balance of component A is :
xp F = yp,avg. D+xwW (137)
Though the simple or differential distillation as a method of separation is not effective,
many such units are used, especially where the components to be separated have widely
ee boiling points and methods giving sharp separations are not necessary.
Cor
nstant Relative Volatility: \
I During the course of distillation, although the temperature in distillation still/kettle
increases, the relative volatility does not change much and so some average volatility «
can be used, over the concentration range involved, which makes the direct integration of
RHS of Equation (1.36) possible and graphical integration can thus be avoided.
The relationship between the composition of vapour (y) and that of liquid (x), in
equilibrium, in terms of relative volatility is
y = awl+(a-1)x
So y from above Equation can be substituted in Equation (1.36).
wee foe
Wer tyes
Xp
m= =_—-
WwW Ox
*W 1+@-Dx *
XP
F 1+(a-1) x] dx
aw * J Gress ee)
Xw
Consider the term wot of RHS of Equation (1.38).
l+#(a-1)x sd ¢ox-x
ox—x[1+(a-1)x] ~ ox—-x-ax?+ x?
_ (=x) sax
* x@-D-x @-D
_ (= +ux
* (a-1) &— x?)
(=x) + ax
* (@-1)x(-x)Mass Transfer — I 4.11 Distillation
a
a-1
(=x)
xd-»*
1a
x*I-x
Putting the above value of RHS back into Equation (1.38), we get,
XP Xp
J parva i
xw x
Ww
1-xp
ox
x(1-
“a-1
Integrating we get,
E
ine [in Zt ain =*|
Equation (1.39) relates F, W, xp and xw through a.
Equation (1.39) can be arranged in another useful form as :
Add and subtract In [(1 — xw)/(1 - xp)] in bracket on RHS of Equation (1.39).
++ (1.89)
F_i1[),% 1-xw 1-xw 1-xp
ny - gi [sees 2 lap -angae|
Combining and rearranging the terms in bracket,
ad xp (1 xw)
hy = A [nes
Fool xp (1 - xw) 1
ng = aim? eal
Fol xpd —xw) 1 xy
Inge = aa ade * Tome ... (1.40)
This can be rearranged to another form as :
Fo. i-xy 1 xp (1— xy)
=~ “ise, 6-1 “gon -o
wl. . 1 jy er (1 -xw)
NW(1l-xw) ~a@-1 xw(l-xp)
(@-Din FQ=2p) f jn Xe-2w)
W(-xw) xw (1 — Xp)
qin FO=¥8) my FU=xe) 2 ty Xe(L-2w)
" W—xw) Wd -xw) xw (1 — xp)
gin FQ-x5) 2 jp xe(-xw) 4, FO-xp)
W(1-xw) xw( xp)" W(—xw)
ain FG) . pe wetheme Bi oe
W(-xw) xw(l—xp) W(1-xw)
gin FQ-xp) 2.) Fur
Wd-xw) W xw
| in FRE. FQ -xp) | 1. (14)
Wxw
oln Wa xw)Mass Transfer — II 4.42 Distillation
Equation (1.41) relates the number of moles of A remaining in the residue, W xy to that
of B remaining, W (1 - xw).
F xp = number of moles of A initially, let it be Noa
F(1-xp) = number of moles of B initially, let it be Nop.
W xw = number of moles of A remaining, let it be Nq
(after distillation is over)
W (1-xw) = number of moles of B remaining, let it be Np.
Noa _ Nop
Ine = ain se
Noa _ (Nos\*
Na ~ (Ne
Nay® _ Na
(Bos) * Noa
Np. Na)
Na _ (Na vee (1.42
Nos (a) 2
Differential Condensation :
In this case, vapour feed is slowly condensed and condensate is drawn in equilibrium
with vapour residue. Let F be the moles of vapour of composition yy and D be the moles of
vaporous residue of composition yp then the treatment similar to that described above yields
F_Pa
me = foe .. (1.43)
yp 27 *
Flash or Equilibrium distillation :
Flash distillation is normally carried out in continuous manner. In this method, a
liquid mixture is partially vaporised, vapour and liquid are allowed to attain equilibrium
and finally withdrawn separately.
Vapour
‘fr mole,
y
Heat exchanger
Separator
Liquid
(=f) mole, x
Fig. 1.5: Flash/Equilibrium distillationMass Transfer - II 4.13 Distillation
Feed is heated in a tubular heat exchanger. The hot liquid mixture is then fed to a
separator via pressure reducing valve whereby pressure is reduced and vapour is formed at
the expense of liquid adiabatically. The liquid is withdrawn from bottom of the separator
and the equilibrium vapour leaves the separator from top which is then liquified in a
condenser. Flash distillation is commonly used in petroleum industry, handling
multicomponent system in the pipe stills.
Consider one mole of liquid mixture, having xp mole fraction of more volatile
component, is fed to flash distillation unit. Let f be the fraction of feed that is vaporised and
is of composition y. Then (1 — f) will be the moles of residual liquid obtained. Let x be the
mole fraction of more volatile component in liquid.
Then, material balance of more volatile component gives :
xp = fry+(1-fx
fy = -(-Ox+xp
ys tat te (1.46)
Equation (1.46) is a material balance/operating line for flash distillation with slope
equal to - (1 — f/f and intercept equal to xp/f.
The point of intersection of operating line and diagonal (x = y) is,
G-fx x»
- -250% ,8
ey
GPx,
scares 2
xf = -xtxf+ xp
. x =
and y =
For f =1, feed totally vaporised (feed 100 mole per cent vaporised)
Slope = - 452-0
and hence operating line is parallel to x-axis through point (xp, xp) on diagonal.
For f = 0, no feed is vaporised.
Slope = > and operating line will be parallel to y-axis through point (xp, xp) on
diagonal.
The operating line for various values of f on equilibrium diagram is as shown in
Fig. 1.6.
1
WZ
0,0 x—> 1
Fig. 1.6 : Plotting the material balance line (operating line) for flash distillation on
equilibrium diagramMass Transfer — Il 1.44 Distillation
09 x—> 1
Fig. 1.7 : Determination of x and y for a given f
Fig. 1.7 shows method of obtaining equilibrium compositions of vapour (y;) and
liquid (x;) for a given f.
Continuous Rectification - Binary Systems :
Rectification is commonly encountered in industrial practice as it is possible to get
almost pure product by this method.
The enrichment of the vapour stream as it passes through the column in contact with
reflux is termed as rectification.
In this separation method, part of the condensed liquid is returned back as a reflux and
maximum enrichment of more volatile component in vapour is obtained by successive
partial vaporisation and condensation by multistage contact of vapour and liquid. This is
achiéved in a single unit called as fractionating column.
wo mating Column :
Fractionating column or fractionator consists of (i) cylindrical shell divided into
sections by a series of perforated trays, (ii) reboiler and condenser. The liquid
mixture to be separated is introduced in the cylindrical column more or less centrally, The
column itself is divided into two sections - rectifying and stripping section. The section
above the feed plate or tray is called the rectifying section, wherein vapour is washed to
remove the less volatile component with the liquid returned to the column from top (known
as reflux). The rectifying section is also called the enriching section as the feed is
enriched in this section, owing to which the top product/distillate is richer in the more
volatile component than the feed. The portion below the feed plate including feed plate is
called the stripping section wherein liquid is stripped off more volatile component by
rising vapour. Perforated trays are nothing but gas-liquid contacting devices on which
gas/vapour and liquid streams are brought into intimate contact for mass transfer to
occur.
The vapours are generated in the reboiler (generally steam heated) and are fed to the
bottom of the column. The liquid removed from the fractionator rich in less volatile
component is called bottoms or bottom product. The vapour issuing from the top of column is
fed to the condenser where latent heat is removed with the help of circulating coolant
through the condenser. A part of condensed liquid is returned to the column (reflux) and
part is withdrawn as a top product or distillate which is rich in more volatile component.
As we move up the column, vapour becomes richer and richer in more volatile component
and as we move down the column, liquid becomes richer and richer in less volatile
component. As the liquid is at its bubble point and vapour is at its dew point, temperature is
maximum at bottom and minimum at top.
7Mass Transfer — I 1.15 Distillation
Condenser
7 J Accumulator
El y
=
Cooler
(
Pr Distillate
Xp
Plate
Feed (F), F-----4
:
Fo be----4
oer.
|---- 4. vapour
‘Reboiler
Liquid Steam in
Condensate
a EN).
Bottom product, xy
Fig. 1.8 : Fractionating column
ication on ideal plate :
Refer to the Fig. 1.9 wherein the plates are numbered serially from top down. Consider
nth plate from top in the cascade. The plate n-1 is immediately above the plate n and plate
n +1is immediately below the plate n. On every plate, the two different fluid streams not at
equilibrium are brought into intimate contact, mass transfer takes place, phases are
separated, and finally two fluid streams leave the plate in equilibrium with each other.
‘Thus, the plate under consideration will receive the liquid Ly_, moles/h of composition
Xp-1 and the vapour Va41 moles/h of composition yp+1 from plates n-1 and n+1
respectively. The liquid Ly moles/h of composition x, and vapour Vj moles/h of
composition yn leave this plate for plates n+1 and n -1 respectively in equilibrium with
each other.
When vapour from plate n+1 is brought into intimate contact on plate under
consideration with liquid from plate n-1 and (the diffusing substances distribute
themselves between the phases) their compositions tend to change to attain equilibrium
values. During the interchange process, some of the more volatile component is vaporised
from liquid Ly.,, decreasing the liquid concentration from xp_; to Xp; and some of the less
volatile component is condensed from the vapour Vp.1, increasing the vapourMass Transfer ~ II 1.16 Distillation
concentration from n+, to yp. In the column, as liquid is at its bubble point and vapour is at
its dew point, the heat to vaporise more volatile component from liquid is supplied by the
heat released in the condensation of less volatile component from vapour. Thus the net
effect is that the more volatile component is transferred to the vapour rising up from the
liquid running down the column, while the less volatile component is transferred to the
liquid running down from the vapour rising up the column. Liquid and vapour phase
composition increases along column height with respect to more volatile component and
therefore temperature decreases. The temperature of plate n is less than that of the plate
n+ 1 and greater than that of the plate n - 1.
ty, 1
Plate n- 1
Plate n @
a
5
2
Platen+1 0,0 AC DB 1.0
| oe
Va+2
e = xy Caxy,
2 D= ues Bay
Fig, 1.9 : Material balance over ideal plate Fig. 1.10 : Boiling point diagram showing
2 rectification on an ideal plate
Material balance :
Consider that the column is fed with F moles/time of liquid mixture (feed) with xp mole
fraction of more volatile component. Let D moles/time of composition xp are withdrawn as
a distillate and W moles/time of composition xy are withdrawn as a bottom product.
Overall material balance :
Feed = distillate + bottom product
F =D+W ws. (47)
Material balance of more volatile component (A) over fractionator :
Ain feed = A in distillate + A in bottom product.
xp F = xp D+xwW + (1.48)
With the help of Equations (1.47), and (1.48), it is possible to calculate D and W
Imowing F, xp, xp and xy.Mass Transfer — 1! 1.17 Distillation
Eliminating W from Equations (1.47) and (1.48), we get,
DIF = (xp -xw)/(xp -¥w) (1.49 a)
Eliminating D gives
WIE = (Xp — xe)/(tp — xw) va (1.49 b)
Let L be the moles/time of liquid returned to the top of column then,
Reflux ratio = R
This reflux ratio is also known as external reflux ratio.
IV is the (moles/time) molal flow rate of vapour leaving the top of column then, the
ratio L/V is known as internal reflux ratio.
Vv
~ Condenser
ee
+——— 4;
D. Xp
Tt:
L, Vas
Xn Yael
Fig. 1.11 : Rectifying section including condenser
palance around condenser:
Vv =L+D
o L =vV-D ++ (1.50)
and D=V-L
Overall material balance over Fig. 1.11 is:
Vapour flow to platen = liquid flow from plate n + distillate withdrawn
Vat1 = Int+D + (61)
Similarly, material balance of more volatile component (A) is:
Vn+i¥nt1 = Ln ¥n +D Xp + (1.52)
In , , Dx
Yor = Vas * Vas
Dxp
Yor. = Vy, * Vane ++ (1.58)
From Equation (1.51),
Vater = Int+D
Therefore Equation (1.53) becomes :
.. (1.54)Mass Transfer — Il 1.18 Distillation
Equation (1.54) is known as the material balance line or operating line of the
rectifying section,
V,
n+ 1°¥m +1
Plate m +1
G Reboiler
ee
Fig. 1.12 : Stripping section including reboiler
Overall material balance over Fig. 1.12:
Liquid flow to platem +1 = Vapour flow from plate m + 1
+ Bottom product withdrawn
Lm = VmeitW vos (1.55)
Similarly,
Material balance of more volatile component (A) :
Lm Xm = Vine ¥m+it W Xw (1.56)
Rearranging the Equation (1.56),
Lm Wxw
Ye = ym yo 5D)
We know from the Equation (1.55), that Vinex = Lm- W
ie
= Ww (2.58)
en aw ew)
‘The Equation (1.58) is known as the material balance line or operating line of the
stripping section.
Analysis of fractionating columns :
The theoretical/ideal stages/plates required for a given degree of separation can be
obtained by :
1. McCabe - Thiele method.
2. Lewis - Sorel method. ,
3 Ponchon — Savarit method.
McCabe - Thiele Method :
It is a graphical procedure of obtaining theoretical plates
Assumptions underlying the method are :
1. Constant molal heat of vaporisation.
2. No heat losses.
3. No heat of mixing.Mass Transfer — Il 1.19 Distillation
Consider any plate n in the rectifying section.
Va r
an
Viet
Fig. 1.13
A heat balance across plate n is
Unt Hig ,+Vnei Hy,,; = Ln Hi, +Vn Hy, + heat losses + heat of mixing
Heat losses are negligible for good insulation.
Heat of mixing is zero for ideal system.
Una Hig j+Van Bvgy = In Hig +¥n Hy
Hy and Hy ~ enthalpies of liquid and vapour per mol.
If the molar heat of vaporisation is constant (independent of the composition) then
one mol of vapour Vn; on condensing releases sufficient heat to liberate one mol of vapour
Vp. It follows that V, = Vns1. Therefore, the molar flow of vapour up the column is
constant. As the temperature change from one plate to the next is small, H,,, can be taken
equal to Hy,
Ina Hi, +Von Hy,,, = VauHy,, *%n Hy,
” Ina = In
So the moles of liquid reflux in this section are also constant.
Therefore, Ly and Vp41 are constant in the rectifying section and Vin, 1and Lm are
constant in the stripping section.
ie. molar flow rates of vapour and liquid are constant in each section of the column.
In = Ina=L, Im=bma =U
Vn = Van=V, Vma=Vm =V!
[The above cited assumptions lead to a concept of constant molal vapour flow and
constant molal liquid flow in any section of the column. In other words, for one mole of
vapour condensed, one mole of liquid is vaporised. Thus Vp = Vneu In =Ln+1 --- ete]
The subscripts n, n + 1, m, m +1... etc. may be dropped and the operating lines then
plotted on equilibrium diagram are straight.
‘The operating line of the rectifying section becomes :
4 L Dxp
*gpeen .. (1.59)
AsR = , above equation becomes :
Xp
y Reix* tees ++ (1.60)Mass Transfer ~ I! 1.20 __Distilation
Point of intersection of the operating line for the rectifying section and the 45° diagonal
(x = y) obtained as,
R xp
Y= Rei **Re1
Putting y=x
x
x Rai Ren
(R+I)x = Rx+xp
x = x
and y =X
‘Thus, the operating line of the rectifying section is to be drawn on equilibrium
diagram through the point with the coordinates (xp, xp) on the 45° diagonal and with the
slope equal to R(R + 1) or intercept on y-axis equal to xp/(R + 1). 7
The equation of the operating line of the stripping section becomes :
L! W xw
2 S ... (161)
Y..56gta Woe (1.61
The point of intersection of the operating line of the stripping section and the 45°
diagonal is obtained as follows :
W xw
L'-W
Diagonal :
Thus, the operating line of the stripping section is to be drawn through the point having
coordinatés (xy, x) on the diagonal and with the slope equal to py“
Step-wise procedure for obtaining theoretical plates :
1. By material balances, evaluate the terms D, W, L ete.
2. Draw the equilibrium curve and diagonal with the help of x - y data given.
If relative volatility is given, generate the x — y data.
3. Draw the operating line of the rectifying section through the point P (xp, xp) on the
diagonal and with the intercept equal to xp/(R + 1) or Dxp/(L + D) or slope equal to
RR + 1).
4, Draw the operating line of the stripping section through the point M (xw, xy) on the
diagonal and with the slope equal to 75.
5. Starting from (xp, xp) on diagonal, draw a horizontal line to meet the equilibrium
curve at point ‘a’. Drop a vertical from point 'a' to meet the operating line at point 1.Mass Transfer - Il 1.21 Distillation
TP (Xp: Xo)
Line - 1 - Rectification Section
Line - 2 - Stripping Section
y
Intercept
0,0 wx — 1.0
Fig. 1.14 : Determination of theoretical plates by McCabe - Thiele Method
6. Proceed in this way, that is constructing the triangles (representing the stages)
between equilibrium curve and operating line of rectifying section, till we are
above the point of intersection of two operating lines. Once we cross this point of
intersection, construct the triangles between equilibrium curve and the operating
line of the stripping section i.e. dropping the verticals on the operating line of the
stripping section.
7. Proceed in the same manner till we reach exactly or cover the point M (xw, xw)-
8. Count the number of triangles between xp and.xw. Each triangle on x - y diagram
represents a theoretical plate.
9. If number of triangles are 'n’, then 'n' represents the theoretical number of plates
including reboiler and n - 1 represents the number of theoretical plates in a
umn to achieve the desired degree of separation.
sain ot si -Thiele Method :
7 1, Ibis not used when relative volatility is less than 1.3 or greater than 5.
2. It is not used when more than 25 theoretical stages/plates are required, and
3. It is not used when operating reflux ratio is less than 1.1 times the minimum reflux
ratio.
2, Lewis-Sorel Method of Determination of Number of Theoretical Stages/Plates :
‘The equation of operating line of the rectifying section is :
Dxp
ae
You = Trp +igeD wa (1.62)
‘The equation of the operating line of the stripping section is :
w
tn = ... (1.63)
yati = TW "Law
1. From the data cited in problem, evaluate the terms - D, W, L ete.| Mass Transfer-N 4.27 Distillation
Vapour leaving the partial condenser has @ composition yp [Refer Fig. 1.19 (b)] which is
in equilibrium with xc, composition of liquid reflux.
Operating line for rectifying section with total condenser is :
Yner = (RR+ 1) xy +Xp/R4+1
Operating line for rectifying section with partial condenser is :
yout = BR+1)¥n +yp/R+1
only difference is xp is replaced by Yp-
This operating line passes through point (yp, Yn) on the diagonal where yp is the
composition of distillate withdrawn (in vapour state)
As ypis in equilibrium with xc, the partial condenser is represented by triangle aba’.
‘As far as the column is concerned, the operating line ends at point a’ with coordinates
(xc, y1) and triangle a’b'c! represents the top plate in the column.
In case of partial condenser, we have to adopt the same procedure of construction of
stages as that described previously for total condenser [only difference is xp is to be
replaced by yp~ (composition of vapour produet)] and count the number of stages between yp
and xy. Total number of theoretical plates counted starting from yp to xw will include
reboiler as well as partial condenser (each of them acting as one theoretical stage).
Number of theoretical plates counted between yp and xw =n +2.
n+2-2
Number of theoretical plates required in column =
For example, suppose we counted 10 theoretical plates between yp~xw (i.e, including
partial condenser and reboiler) then
Number of theoretical plates
required (in the column) (n+2)-2
10-2=8
(as the reboiler and partial condenser are both equivalent to one theoretical plate.)
jux Ratio:
1. Infinite reflux ratio or total reflux ratio, R..:
‘The total reflux operation is of interest to know the minimum number of plates
required (it sets lower limit on number of plates required) and is not a practical method of
operation as at total reflux the product rate is zero.
‘A column operating under total reflux is shown in Fig. 1.21. In this case, enough
| material is charged to a distillation assembly and column is operated under total reflux.
During the operation of the column, vapours issuing from top are condensed and all
condensed stream is fed back to the column as reflux. Also all liquid going to the reboiler
'
'
j
is vaporised and is fed to the column. Thus, under the condition of total reflux P = 0, D = 0
and W = 0, therefore Vns1 =m throughout the column. The slope (L/V) of both the operating
Iines becomes unity and hence both the operating lines coincide with the diagonal and
tminimam number of stages (theoretical plates) are then required for the desired degree of
separation (xp — xy). Total reflux operation corresponds to maximum reboiler heat supply
and condenser cooling capacity for the separation,Mass Transfer ~ II 1.28 Distillation |
=
1
2
3
Qe 4 |
- Fig. 1.21: Operation under total reflux
4, Minimum Reflux Ratio, Rm :
At total reflux, the operating lines of both sections coincide with the diagonal and to
effect desired separation, number of stages (theoretical plates) required are minimum. As
the reflux ratio is reduced, the operating lines move towards the equilibrium curve along
the feed line and the number of stages increase. Ultimately, further reduction in the reflux
ratio results into condition wherein the top operating line touches the equilibrium curve as
shown in Fig. 1.22. The point of intersection of the operating lines lies on the equilibrium
curve and at this point step becomes very close together, so that a zone of nearly constant
composition is formed near the feed plate. Infinite number of plates are then required.
This represents a condition of minimum reflux. Thus, a minimum reflux ratio is that
reflux ratio at which an infinite number of plates are required for the desired separation.
At minimum reflux ratio, the requirement of heat supply to the reboiler and that of coolant
supply to the condenser are minimum.
Fig. 1.22 : Minimum Reflux ratioMass“Transfer ~ Il 1.29 Distilation
Calculation of minimum reflux ratio (Rm):
For liquid at its bubble point, the feed line is vertical (parallel to y-axis) and the point C
lies on the equilibrium curve and has the co-ordinates (xp, yr)-
Draw the equilibrium curve and diagonal and draw the feed line, a vertical through the
point P (xp, xp) on diagonal. Point of intersection of the feed line with the equilibrium
curve is also a point of intersection of the operating lines at minimum reflux.
Operating line
(rectification: section)
0,0 eh 10.
Fig. 1.28 : Method of obtaining R,, (saturated liquid feed)
Slope of the operating line AC is given as :
m_ _ *p- Je = (1.79)
Ra vl % xp=2r :
Rm (xp- Xr) = (Rm + 1) p-yr)
Rm Xp- Rm Xr = Rm Xp - Rm yr+ XD YP
Rm (vr- X) = XD-YF
Rm = aE .-- (1.80)
Yr- Xr
Similarly for feed as a saturated vapour, the feed line is horizontal.
Slope of the line AC is given as :
4. oe (81)
Rm+i ~ xp-x
| f
Rm ;
- (1.82)
Fig. 1.24: R,, for saturated vapourMass Transfer ~ Il 1.30 Distillation
For feed as a cold liquid : i
. for ‘q! values greater than one :
Rm = 2=% (1.88)
v ~x
x—>
0,0 J
Fig. 1.25 : 'R,,' for cold liquid
For 'q' values less than one and greater than zero :
Slope =
+ (1.84)
1.0
0,0
Fig. 1.26 : 'R,,' for feed-partially vapour
3. Optimum Reflux Ratio:
Any reflux ratio between infinite reflux ratio requiring minimum number of plates
and minimum reflux ratio requiring infinite number of plates is a workable system
which requires finite stages for desired degree of separation. At minimum reflux ratio as
infinite number of plates are required, fixed cost is also infinite while cost of heat supply to
reboiler and condenser coolant is minimum. As the reflux ratio is increased, the number
of plates decreases and the fixed cost decreases at first, passes through a minimum and
then increases as with higher reflux ratio the diameter of the column and sizes of reboiler
and condenser increase. The operating cost increases continuously as the reflux ratio is
increased as it is directly proportional to (R + 1). At total reflux, though the number of platesMass Transfer - Il 1.31 Distillation
are minimum, the cost of heat supply to reboiler and condenser coolant is maximum and
4
N
a
“(I
R, a
Fig. 1.27 : Relation between reflux ratio and number of stages for distillation
also large capacity reboiler and condenser are needed. The total cost which is sum of fixed
cost and operating cost also decreases to a minimum and then increases with reflux ratio.
The optimum reflux ratio occurs at a point where the sum of the fixed cost and operating cost
is minimum, The optimum reflux ratio is defined as that reflux ratio at which the sum of
the fixed cost and operating cost is minimum. As a rough approximation, the optimum
reflux ratio is usually 1.1 to 1.5 times the minimum reflux ratio.
Operating costs
Cost Fixed costs
Rm)
R (Reflux ratio) —>
Fig. 1.28 : Optimum reflux ratio for distillation
Fenske - Underwood Equations:
Minimum Reflux Ratio (Rm) : The minimum reflux ratio, requiring infinite number
of plates, ean be obtained analytically when the relative volatility is taken as constant over
the concentration range concerned (xp ~ xw)- So let us obtain the required relationship
with which we can calculate Rm.
For the normal equilibrium curve which is concave downward throughout its length,
the operating line of rectifying section, at minimum reflux, passes through the point of
intersection of the q-line and the equilibrium curve.
"The equation of operating line for rectifying section dropping the subscripts is :
x+oe + (1.85)
a
Y "RelMass Transfer ~ II 1.75 Distillation
Outlet weir
Inlet weir
Lf comm
/
Tray
‘Down
conier
Seal pot
Fig. 1.61 : Downcomer - weir seal plot
Entrainment :
As gas/vapour bubbles through the pool of liquid on a plate, a large amount of turbulence
is set up and the liquid particles can be entrained by the rising gas. Carry over of liquid
articles by rising gas from a plate below to the plate above is known as entrainment and is
much more pronounced at high gas flow rates. Entrainment reduces the concentration
change per plate and hence, decreases the plate efficiency. Tray spacing, vapour flow rate,
depth of liquid on tray are the factors on ~—e of entrainment depends.
PACKED COLUMNS FOR DISTILLATION:
For distillation operation, packed columns are especially useful whenever wé have to
‘carry out operation at low pressure (vacuum distillation) and whenever we are dealing
with heat sensitive materials. Packed columns are cheaper than plate for column diameter
less than 600 mm. A packed column consists of a cylindrical shell filled with some sort of
ackings (rings or saddles) which offer large interfacial area for mass transfer. A
mmon arrangement of the packed column for distillation operation is shown in Fig.
1.62, wherein the vapour flows upward and the refluxed liquid flows downward giving
tinuous contact.
The ability of a given packing to effect the desired mass transfer between gas and
liquid phases (i.e. to effect the desired degree of separation) is usually expressed in an
empirical form, as the height equivalent to one theoretical plate (HETP). In case of plate
eolumns wherein a process of enrichment is stage wise, vapour leaving the plate is richer
ith respect to more volatile component than vapour entering the plate by one equilibrium
ge. In packed columns, the same enrichment of vapour will occur in a certain height of
packing which is termed as height equivalent to one theoretical plate or height equivalent to
theoretical plate. Thus, in packed columns, one equilibrium step is represented by a
rtain height of a packed bed and the required height of packing for the desired degree of
paration is given by : HETP x number of ideal plates required. HETP is defined as the
ight of packing (packed bed) giving the enrichment of vapour same as that can be
ained by one theoretical plate (in stage-wise operation).Mass Transfer ~ Il 1.76 Distillation
Condenser
Vapour
Accumulator
Reflux
tH Distillate
Packings
Fea} | — Distributor
A Reboiler
Steam
Condensate
Boitoms
Fig. 1.62 : Packed column for continuous distillation
‘The HETP can be estimated with the help of an empirical equation such as
HETP = ky: G2-DP - 218 +a - wp «.. (1.160)
where ky, kp and ky are empirical constants for packing and are function of type and size of
packing.
G — Superfacial gas mass velocity
Dt - Tower diameter
Z - Height of packing
a — Relative volatility
uy and p, are viscosity and density of liquid respectively.
The HETP is an experimental quantity, characteristic of each packing and depends on
the type and size of the packing, flow rates of each fluid and concentration.
Method of Transfer Units :
Fractionation by means of a packed column involves continuous countercurrent
contact of the vapour and liquid whereas fractionation by means of a plate column involves
stagewise contact of the vapour and liquid. So in the packed column there is a continuous
change in the composition of the components and in the plate column there is a
discontinuous change in the composition of components (effected at each plate).
The theoretical unit of separation in a packed column is the transfer unit and not the
theoretical plate (as it in a plate column). The efficiency of a packing consequently can be
measured as the height of packing to give a separation of one transfer unit (height of
transfer unit).Mass Transfer ~ Il 1.77 Distillation
‘The height of a packed column can be based on the number of transfer units and the
height of transfer unit. The height of a packed column can easily be obtained by
multiplying the number of transfer units by the height of transfer unit.
7, = Number of transfer units x height of transfer unit.”
‘The number of transfer units is the measure of ease or difficulty of separation. More
difficult the separation, the more such units would be required. Hence, if very high purity
products are desired or for high degree of separation, a large number of transfer units will
be required.
‘The height of transfer unit is a measure of the separation effectiveness of a particular
packing for the chemicals being processed. If the rate of mass transfer is high and surface
avea for mass transfer is large then the height of transfer unit is small. For determination
of the height of transfer unit, we require a knowledge of mass transfer coefficients in units
consistent with those in which the composition of phases is expressed.
Consider a packed column as shown in Fig. 1.63 in which the composition of the more
volatile component increases from yp to yt-
Y:4To condenser
Je—— Reflux
Vok t
Fe .
Feed-—>
“EF
Vapour Liquia
from reboiler _to reboiler
Fig. 1.68 : Packed column for distillation
Let A be the empty column cross-sectional area, Z be the height of packed section ofa
column, ‘a’ be the active interfercial surface per unit volume of packing (interfacial area
per unit volume of packing).
Consider a differential element of height 4Z, through which two phases pass
countereurrently, wherein a differential change in vapour composition, dy, takes place.
‘At a same time, a differential change in liquid composition is dx.
For steady-state operation, material balance of the more volatile component A over the
differential height aZ assuming constant molar overflow i.e. neglecting change in molar
flow rate in any particular section is
Vdy = Lex ... (1.161)
where V is the vapour flow rate in enriching section of the column in moles/time and L is
the molar flow rate of liquid in mole/time. V is constant in the entire enriching section.
Tt will be also constant in the stripping section but of different magnitude depending upon
the feed conditions.
Fach term of Equation (1.161) is the indication of moles of A diffusing i.e. rate of
addition or depletion of A to the vapour phase or from the liquid phase and is a statement of
the rate of transfer of A across the transfer area in dZ. This must be equal to the total
driving force divided by the total resistance.Mass Transfer - II 1.78 Distillation
So the rate of change of a component A within the phase must be equal to the rate of
transfer to the phase.
‘Thus, for V-phase (vapour phase) :
Vdy = kg (yj-y) dS = Kg (y*-y) dS we (1.162)
where dS is the interfacial transfer area associated with the differential column height dZ.
dV = differential volume of packing in height dZ = AdZ
dS = differential interfacial area for mass transfer = aAdZ
in height dZ
Vdy = kg (i-y) aA dZ=Ke (y"—y) aA dz
Vady = kga(yi-y)AdZ =Kgaly*-y)AdZ +. (1,168)
where (yj — y) is the driving force over the gas film
(y" -y) is the overall driving force for the gas phase/vapour phase - (overall driving
force in terms of vapour composition).
Ke is the overall gas phase mass transfer coefficient in mol/(time)-(unit driving force)
Kg «a is the volumetric overall mass transfer coefficient in mol/(volume) - (time)
(unit driving force).
In distillation operation, vapour and liquid compositions are expressed in terms of
molefraction, so units of Kg-a will be mol/(volume) - (time) - (molefraction).
Use of Kg - a requires the gas phase composition (y*) in equilibrium with the bulk
liquid composition and use of kg * a requires the gas phase composition (y;) at the interface.
It is possible only to measure the bulk composition and determination of interface
composition is ordinarily impossible.
: Vay = Kgaly"-y)AdZ ++ (1.164)
(WA) dy = Kga(y*-y) dZ
agi Hs ]
-¥.
Ke aly
Integrating between limits,
‘ os WA (_4@:
Je = | ae)
: yb
The molar flow rates (V and L) are assumed to be constant in enriching section. The
overall mass transfer coefficient is a function of these phase flow rates. If the physical
properties do not vary appreciable, Kg is also a constant.
Fi wa 7 a
wa=ee fo
‘ Ko di.s5 >
yt
z = WA { ay (1165)
Koay y'-y
In Equation (1.165), the integral term represents the integrated ratio of the change in
vapour composition to the available driving force (in terms of vapour composition) tendingMass Transfer — Il 1.79 Distillation
to bring this about. This term is defined by Chilton and Colburn as the number of transfer
units (Np. In our present case, Ny is Nog
yt a
y
Nioo = | aos .. (1.166)
‘on J y-7
Niog is the number of overall gas transfer units (i.e, number of transfer units based on
gas phase).
‘The quantity outside the integral of Equation (1.165) is called the height of a transfer
unit (Hp. In present case, Hy is Htgg-
WA
Hos = Kee va (1.167)
Thus, Equation (1.165) can be written as
Z = Hiog* Ntog v.- (1.168)
|A similar series of equations can be written in terms of composition of more volatile
component in liquid phase. The column height can be evaluated using changes in
composition of A in liquid phase and corresponding rate.
Vay = Kea(y’-y)AdZ=Ldx=Kya(x-x)AdZ (1.169)
Ldx = Kpa(x-x)AdZ + (1.170)
where x x" is the overall driving force in terms of liquid phase composition.
Ky, ais the overall volumetric mass transfer coefficient for liquid phase in
mol /( time) « (volume) « (unit driving force).
Ky is the overall liquid phase mass transfer coefficient in mol/(time) « (area) - (unit
driving force).
So for liquid phase, we can write,
dx
x-x"
Nto. = - (L171)
Noy is the number of overall liquid phase transfer units (number of transfer units
based on liquid phase).
Hto. = i «.- (1.172)
Hovis the height of an overall liquid transfer unit.
Hog and Ho, are having dimension of length while Nto. and Ntos are dimension-
less.
Plate Efficiency :
By using either the McCabe-Thiele method or the Ponchon-Savarit method, we obtain
the number of ideal/theoretical/equilibrium stages required for achieving the desired
degree of separation. In case of an ideal stage, the vapour leaving the plate is in
equilibrium with the liquid which leaves it. In actual practice, complete equilibrium is
never reached on any plate. This is due to short contact time and incomplete mixing on
any plate, The vapour leaving an actual plate is usually weaker in more volatile
component than vapour in equilibrium with the liquid leaving it. Thus, for achieving
desired degree of separation in actual practice, we require more number plates than idealMass Transfer — I 1.80 Distillation
plates. To apply either of the methods to an actual case, it is necessary to convert the number
of ideal plates to actual plates. The factor that is used for converting ideal plates into actual
plate is the plate efficiency. The reboiler delivers vapour directly from the boiling liquid
and is thus considered as a perfect plate.
‘Types of plate efficiency :
(i) Overall efficiency/overall plate efficiency — pertains to the entire column.
(ii) Murphree efficiency — pertains to any single plate.
(iii) Murphree local/point efficiency - pertains to a specific location on a given plate.
Overall efficiency is the ratio of number of ideal plates required to produce a given
degree separation to the number of actual plates required to effect the same separation.
theoretical/ideal plates required
To = actual plates required *10
For example, if we need six theoretical plates to effect the desired separation and the
overall efficiency is 60% then the number of actual plates required are 6/0.60 = 10. The
overall efficiency may vary from 30 to 100 percent.
‘The Murphree plate efficiency :
It is the efficiency of any single plate based on vapour phase composition.
For the nt® plate in the column, the Murphree efficiency is given by
Yn-Yau
mM = oe
Y_7Yne
where, _Yp is the average composition of vapour leaving plate.
Yne1is the average composition of vapour entering plate
y,, is the composition of vapour in equilibrium with liquid leaving plate.
It applies toa individual plate in a column and is defined as the actual change in
average vapour composition achieved by a given plate divided by the change in average
vapour composition if the vapour leaving the plate were in equilibrium with the liquid
leaving the plate. This efficiency is less convenient to use as it involves plate to plate
compositions rather than the terminal compositions.
Point/Local efficiency : It pertains to a particular place on the plate surface (applies to
single location on a given plate). It is defined by
1 _ Yn, local ~ Yn+1, local
Yiocal ~ Yn+1. local
where — Yn, local is the composition of vapour leaving specific location on plate n
Yn ts local is the composition of vapour entering plate n at the same location.
Yiocal 18 the composition of vapour in equilibrium with the liquid at the same
location (i.e. in equilibrium with xIocal)-
‘To obtain satisfactory plate efficiencies, it is highly necessary that the plates must
operate properly. Adequate and intimate contact between vapour and liquid is essential.
Each of the unfavourable phenomena such as entrainment, excessive foaming, weeping,
short-cireuiting and flooding lower the plate efficiency.Mass Transfer — II 1.81 Distillation
SOLVED EXAMPLES
Ex.1.1: A mixture containing benzene and toluene with 40% benzene and 60% toluene
is to be separated in a fractionating column to give product containing 96% benzene and
bottom product containing 95% toluene. Feed is a mixture of two-third vapour and one-third
liquid, Find out the number of theoretical stages required if reflux ratio of 1.5 times the
minimum is’ used.
Data: Relative volatility ots = 2.5
Solution : Basis : Feed containing 40% benzene and 60% toluene by weight.
Molecular weight of benzene (CsHs) = 6x12+6x1= 78
Molecular weight of toluene (CsHsCHs) = 7x12+8x1=92
In 100 kg of feed there are 40 kg of benzene and 60 kg of toluene.
Molefraction of benzene in feed = xp = wets
044 ~
Distillate contains 96% benzene by weight.
. cor 96/78
Molefraction of benzene in distillate = x» = 9g7g4 4 = 096 «
Bottom product contains 95% toluene and 5% benzene by weight.
: . B78.
Molefraction of benzene in bottom product =xw = g77g 4 gg/a = 0.058
Gap = 2.5
Generate x-y data with the help of equation :
¥ = T+@-Dx
1 and evaluate corresponding y value:
Plot the equilibrium curve.
Procedure to determine the minimum reflux ratio (Rm) :
q is the fraction of the feed that is liquid. Feed is two-third vapour and one-third liquid,
so 1 mole of feed results in 1/3°4 mole of saturated liquid in the stripping section.
q=13 = 0.333
or q = 1~f, where fis fraction of feed that is vaporised
= 1-28 =1-0.667 = 0.333
Slope of feed line =
Slope = tan @
e
Intercept on y-axis
0.44 / (1 - 0.333)
= 0.66Mass Transfer — I! 1.82 Distillation
Draw the feed line through the point Q (0.44, 0.44) on the diagonal with slope equal to
— 0.5 (8 = — 26.569) or with intercept on y-axis equal to 0.66 to cut the equilibrium curve at
point P. Read y' and x' as the coordinates of point P.
From graph, y' = 0.51 and x' = 0.295.
Minimum reflux ratio for feed partially vaporised is given by
f= OY
Rm = yg!
0.966 - 0.51
Rm = 051-0295 = 22
Operating reflux ratio= R = 1.5 Rm = 15x2.12 =3.18
Operating line of the rectification section :
It has point (0.966, 0.966) on the diagonal and intercept on y-axis
= xXp(R+.1) = 0.966/(3.18 + 1) = 0.231
Draw this line through M (0.966, 0.966) on the diagonal with intercept of 0.231 on y-axis,
Draw the operating line of the stripping section through the point (xw, xw)
N (0.058, 0.058) on the diagonal and passing through the point of intersection of q-line i.e.
feed line and operating line of the rectification section. Do step-by-step construction
between equilibrium curve and operating lines starting from the point M (0.966, 0.966) and
reaching exactly or covering the point N (0.058, 0.058) and count the plates.
Number of theoretical plates including reboiler =n = 11.
Number of theoretical plates required in the column =n-1 = 11-1 = 10 ... Ans.
0.9
08
07
06
yo
0.5
onl Q.RS.O. line
03
x
02
5.8.0. line.
0.231
On Pit iat
N (0.058, 0.058) tas
00°01 02 03 04 05 06 07 08 09 1.0
x—
Fig. E 1.1: Graphical construction of ideal stagesMass Transfer — Il 1.83
Distillation
Ex. 121A mixture of 35 mole % A and 65 mole % B is to be separated in distillation
column. The concentration of A in the distillate is 93 mole % and 96 mole % of all A is in
fistillate, The feed is half vapour and reflux ratio is 4: 1, The relative volatility (on) is
2.5. How many equilibrium stages are required in each section of column ? What could be
the minimum reflux ratio for such operation ?
Solution : Basis : 100 kmol of feed containing A and B.
F = D+W
100 = D+W W =100-D
xp = - = 0.35, Xp = * =0.93
Ain feed = 0.35x 100 = 35 kmol
96 mole % of A is in distillate
Ain distillate = 0.96x35 = 33.6 kmol
Distillate contains 93 mole % A.
Ain distillate
Mole %A = ~“Gistillate “10
A in distillate
distillate = (foie % A/100)
Amount of distillate = 228 = 36.13 kmol
Bottom product = Feed — distillate
100 - 36.13 = 63.87 kmol
35 -— 33.6 =1.4kmol
as x100 = 2.2
Bottom product = W
Ain bottom product
Mole % A in bottom product
Chéck :
Mole % B in bottom product 100- 2.2 = 97.8
B in distillate = Distillate — A in distillate
36.13 — 33.6 = 2.53 kmol
u
|
Bin feed
B in distillate + B in bottom product
0.65x100=65 = 2.53 + 0.978 x 63.87 = 64.995 ~65
D = 36.13 kmol, W = 63.87 kmol, xp = 0.35, xp = 0.93, xw = B = 0.022, on = 2.5.
a
Y= T¥G@-Dx
Take x =0, 0.1, 0.2 ... 1.0 and evaluate y and tabulate the data.
x]0 ] 01] 02 | 03 [ 04 [ 05 | 06 | 07 | 08 [ 09 | 10
y [0 | 0217 | 0385 | 0.517 | 0.625 | 0.714 [0.789 | 0.854 | 0.91 [0.957 | 1.0
G)_ Plot the equilibrium data and diagonal.
(ii) Plot the q-line.
Feed is half vapour (given), so feed is half liquid.
fraction of feed that is liquid
0.5, (q =0.5/1 =0.5)
q
q
slope of q-line =
slope =
Xp =